# US 10,441,930 B2 · Method for producing pulverulent solids from alkali salts of silanols

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- Number: US 10,441,930 B2
- Document ID: US10441930B2
- Status: Granted
- Kind: B2
- Application number: 15/557,112
- Filed: 2016-02-19
- Published: 2018-02-15
- Granted: 2019-10-15
- Earliest claimed: 2015-03-10
- Assignees: Wacker Chemie AG
- Applicants: Wacker Chemie AG
- Inventors: Michael Stepp; Daniel Schildbach
- Web page: https://patentgrep.com/patent/US10441930B2

## CPC

- B01J 2/04: in a gaseous medium {(if combined with suspending the material in a gas, e.g. fluidised beds B01J2/16)}
- C04B 24/42: Organo-silicon compounds
- C04B 28/02: containing hydraulic cements other than calcium sulfates
- C04B 28/14: containing calcium sulfate cements {(gypsum-paper plates E04C)}
- C07F 7/1804: {Compounds having Si-O-C linkages (Si-O-acyl linkages C07F7/1896)}
- C09D 5/03: Powdery paints
- C09D 7/63: organic
- C04B 2103/0057: {added as redispersable powders}
- C04B 2103/65: Water proofers or repellants
- C04B 2111/27: Water resistance, i.e. waterproof or water-repellent materials
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)

## Abstract

Pulverulent alkali metal alkyl siliconates having lesser hydroscopicity and improved hydrophobicity in construction materials are produced by spray drying an aqueous solution of an alkali metal alkylsiliconate having a defined range of alkali metal content, a low alcohol content, and a low chlorine content.

## Claims

### Claim 1

A process for producing a pulverulent solid comprising one or more alkali metal organosiliconates, comprising: spray drying an aqueous solution of one or more alkali metal organosiliconates prepared by reacting one or more organosilanes of the formula 1
(R1)aSi(Y)b(—Si(R2)3−c(Y)c)d (1)
or hydrolysis/condensation products thereof, or by reaction of organosilanes of the formula 1 and also hydrolysis/condensation products thereof,
with water and a basic alkali metal salt, and removing liberated dissociation products HY,
where
R1, R2 are each a methyl radical,
Y is hydrogen, F, Cl, Br or OR4 and
R4 is a methyl, ethyl, 1-propyl or 2-propyl group,
a is 1, 2 or 3 and
b, c, d are each 0, 1, 2 or 3,
with the proviso that b+c≥1 and a+b+d=4,
where the amount of basic alkali metal salt is such that there is at least 0.1 mol and not more than 3 mol of alkali metal cations per 1 mol of silicon,
wherein the alkali metal organosiliconate(s) have a molar ratio of alkali metal to silicon of from 0.1 to 3, and prior to spray drying, have a content of alcohol of less than 0.02% by weight, and a content of halide anions of not more than 1% by weight.

### Claim 2 (depends on 1)

The process of claim 1, wherein the basic alkali metal salt is selected from the group consisting of alkali metal hydroxides, alkali metal silicates, alkali metal organosiliconates and mixtures thereof.

### Claim 3 (depends on 1)

The process of claim 1, wherein water is removed in an amount so as to provide a solids content, determined at 160° C., of at least 96% by weight based on the total weight of the pulverulent solid.

### Claim 4 (depends on 1)

The process of claim 1, wherein the alcohol content of the pulverulent solid is not more than 0.05% by weight based on the total weight of the pulverulent solid.